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Preparation method of dialkyl phosphinate

A technology of dialkyl phosphinate and dialkyl phosphinic acid, which is applied in the preparation of dialkyl phosphinate and in the field of chemical synthesis, can solve the problems of product yield decline, complex reaction, difficult purification, etc. Achieve the effects of avoiding the reduction of yield and purity, ensuring yield and purity, and reducing equipment investment

Active Publication Date: 2013-09-25
ZHEJIANG XINHUA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reaction of this method is complicated, and the product obtained is a mixture with complex components, which is difficult to purify, and the product purity is very low, and the productive rate of dialkylphosphinic acid is only 16%.
[0004] CN98811626, CN98811627, etc. disclose to use phosphinate and olefins as raw materials, react to prepare dialkyl phosphinate under the action of initiator, the advantage of this reaction is that can obtain dialkyl phosphinate in high yield products, but must be recovered through complex processes due to the use of organic solvents in the reaction, and undesired formation of telomers due to the high solubility of olefins in organic solvents
Moreover, the presence of telomers and traces of organic solvents in the product can have undesirable side effects on plastics
CN200410104692 etc. disclose the method for preparing dialkyl hypophosphite under the condition of not using organic solvent, but need higher reaction temperature and longer reaction time, and product yield obviously drops
The above reactions all need to be carried out under certain pressure conditions, require high equipment investment, and have certain safety hazards

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Dissolve 300g of sodium hypophosphite monohydrate and 12g of tributyltetradecylphosphine chloride in 1500g of water, then add it to the autoclave, replace it with nitrogen three times, start stirring, raise the temperature to 100°C, and feed ethylene into the reactor In the process, the pressure in the kettle is controlled to be about 0.1MPa by a pressure reducing valve. Dissolve 10g of 2,2'-azobis(2-amidinopropane) dihydrochloride in 100g of water, and continuously and evenly add it to the reaction kettle within 6 hours. After the addition was complete, the reaction was carried out at a constant temperature for 1 hour to obtain sodium dialkylphosphinate.

[0025] Transfer the mixed solution of sodium dialkylphosphinate obtained above into a reactor equipped with a thermometer, stirring, condensing reflux pipe and dripping device, heat to 100°C, and then dissolve 350g of hexadecanohydrate sulfuric acid in 600g of water Aluminum was evenly added through the dropping fun...

Embodiment 2

[0027] Dissolve 300g of sodium hypophosphite monohydrate and 20g of tributyltetradecylphosphine chloride in 1000g of water, then add it to the autoclave, replace it with nitrogen three times, start stirring, raise the temperature to 120°C, and feed ethylene into the reactor In the process, the pressure in the kettle is controlled to be about 0.1MPa by a pressure reducing valve. Dissolve 12g of dibenzoyl peroxide in 100g of water, and continuously and evenly add it to the reaction kettle within 5 hours. After the addition was complete, the reaction was carried out at a constant temperature for 1 hour to obtain sodium dialkylphosphinate.

[0028] Transfer the mixed solution of sodium dialkylphosphinate obtained above into a reactor equipped with a thermometer, stirring, condensing reflux pipe and dripping device, heat to 90°C, and then dissolve 350g of hexadecanohydrate sulfuric acid in 600g of water Aluminum was evenly added through the dropping funnel within 2 hours, refluxed...

Embodiment 3

[0030] Dissolve 350g of potassium hypophosphite monohydrate and 18g of tributylhexadecylphosphine bromide in 1000g of water, then add it to the autoclave, replace it with nitrogen three times, start stirring, raise the temperature to 120°C, and feed ethylene into the reactor In the process, the pressure in the kettle is controlled to be about 0.1MPa by a pressure reducing valve. Dissolve 12g of potassium persulfate in 100g of water, and continuously and evenly add to the reaction kettle within 5 hours. After the addition was complete, the reaction was carried out at a constant temperature for 1 hour to obtain sodium dialkylphosphinate.

[0031] Transfer the mixed solution of sodium dialkylphosphinate obtained above into a reactor equipped with a thermometer, stirring, condensing reflux pipe and dripping device, heat to 100°C, and then dissolve 420g of hexadecanohydrate sulfuric acid in 700g of water Aluminum was evenly added through the dropping funnel within 2 hours, refluxe...

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Abstract

The invention discloses a chemical synthetic method, and specifically relates to a preparation method of dialkyl phosphinate. The preparation method comprises the following steps of: adding a small amount of a reaction auxiliary agent into reaction raw materials including hypophosphorous acid and / or an alkali metal salt of hypophosphorous acid, and dissolving the mixture into water; then transferring the mixture into a pressure kettle; performing nitrogen replacement, and then heating to raise the temperature; introducing alkene, and then adding an initiating agent to react so as to obtain dialkyl phosphinic acid and / or an alkali metal salt of the dialkyl phosphinic acid; and then transferring the dialkyl phosphinic acid and / or the alkali metal salt of the dialkyl phosphinic acid into a reactor, heating to a certain temperature, slowly dropping a solution of a metal salt to obtain a corresponding dialkyl phosphinate deposit, and then filtering, washing and drying to obtain a dialkyl phosphinate product. The preparation method has the advantages that water is used as a reaction solvent system, a specific reaction auxiliary agent is added, and the way of feeding the initiating agent is changed, so that the reaction temperature is lowered, the reaction time is shortened, the product yield and the product quality are improved, and the cost is saved.

Description

Technical field: [0001] The invention relates to a chemical synthesis method, in particular to a preparation method of a dialkyl phosphinate, and belongs to the field of green and environment-friendly flame retardants. technical background: [0002] With people's increasing awareness of environmental protection, safety and health, countries around the world have begun to focus on the research, development and application of environmentally friendly flame retardants. has been widely used. [0003] Dialkylphosphinates as flame retardants can be prepared by various methods. For example, US601172 and CN1280581 disclose taking yellow phosphorus and alkyl halide as raw materials, reacting in the mixed system of aqueous solution of alkali metal hydroxide or alkaline earth metal hydroxide and organic solvent, prepare alkyl phosphinic acid and alkyl phosphinic acid . The reaction of this method is complicated, and the product obtained is a mixture with complex components, which is...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/30
Inventor 应思斌翁志坚刘承伟祝航乔涛钟启刚
Owner ZHEJIANG XINHUA CHEM
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